Réaction #2122506

ord-21951efda33b4875984a232e3799e524

Équation de réaction

[Al+3].[Cl-].[Cl-].[Cl-]
Aluminum chloride
ClC1CCCCC1
cyclohexyl chloride
c1cc(C2CCCCC2)c(C2CCCCC2)c(C2CCCCC2)c1
tricyclohexylbenzene
Rendement 50.7%

Solvants

Conditions de réaction

Température
3°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONAfter the dropwise addition
  2. 2
    workup.STIRRINGthe resultant was stirred at room temperature for 5 hours
  3. 3
    Autrethe obtained reaction solution
  4. 4
    ExtractionThe organic layer was extracted
  5. 5
    Autrethe obtained organic layer was removed by distillation at 40° C. under reduced pressure
  6. 6
    AutreThe resultant was further removed by distillation at 170° C. under reduced pressure
  7. 7
    Températurecooled to room temperature
  8. 8
    workup.ADDITION50 ml of acetone was added
  9. 9
    Autrerecrystallization
  10. 10
    AutreThe precipitated crystals were collected
  11. 11
    Filtrationthrough filtering

Mode opératoire

Aluminum chloride (6.38 g) was added to 20.0 g of benzene, followed by stirring under cooling at 3° C., and 40.4 g of cyclohexyl chloride was slowly added dropwise thereto. After the dropwise addition, the resultant was stirred at room temperature for 5 hours, and the obtained reaction solution was added to ice water. The organic layer was extracted by using ethyl acetate, and the obtained organic layer was removed by distillation at 40° C. under reduced pressure. The resultant was further removed by distillation at 170° C. under reduced pressure and then cooled to room temperature, and 50 ml of acetone was added thereto to cause recrystallization. The precipitated crystals were collected through filtering, thereby obtaining 14 g of tricyclohexylbenzene.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08574814B2uspto-grants-2013_11